CN111171699B - Polyurethane waterproof coating with electromagnetic wave shielding function and preparation method thereof - Google Patents
Polyurethane waterproof coating with electromagnetic wave shielding function and preparation method thereof Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- H05K9/0073—Shielding materials
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Abstract
The invention discloses a polyurethane waterproof coating with an electromagnetic wave shielding function and a preparation method thereof, wherein the polyurethane waterproof coating is prepared from the following raw materials in parts by weight: 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents; the conductive filler comprises one-dimensional conductive filler and two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30). The waterproof coating provided by the invention has good electromagnetic shielding effect, and simultaneously has good comprehensive properties such as extensibility and strength.
Description
Technical Field
The invention belongs to the technical field of waterproof materials, and particularly relates to a polyurethane waterproof coating with an electromagnetic wave shielding function and a preparation method thereof.
Background
Along with the rapid development of electronization and informatization, electromagnetic waves as important carriers for information transmission have penetrated into various aspects of life, and electronic products are more and more widely applied to various fields of national economy and family life, including mobile phones, televisions, household appliances, radars, signal transmitting base stations and signal receiving stations. By using the propagation rule of electromagnetic waves in different media, people can be used for exploration of mineral resources and earthquake prediction. In medical treatment, electromagnetic waves are also widely used, such as physical therapy, diagnosis and treatment of malignant tumors. However, the widespread use of electromagnetic waves creates a complex electromagnetic environment with a number of negative effects, such as electromagnetic interference (EMI), the security of electromagnetic information, and the harm of electromagnetic radiation to human health. Sources of electromagnetic radiation include natural electromagnetic environments, which are derived from the sun's electromagnetic waves and the earth's magnetic field, which are less harmful to humans than man-made electromagnetic environments. Man-made electromagnetic environments generally include: broadcast television, communication facilities, vehicles, electric power systems, household appliances, high-frequency equipment used in industrial research and medical care, and the like. Electromagnetic waves are filled everywhere in a living environment, and the electromagnetic waves can be emitted as long as electrical appliances such as electric fans, microwave ovens and the like are used; an invisible wire in the wall also causes the electromagnetic wave detection pen to beep. The electromagnetic wave of the mobile phone used by people is very strong, and people can find that the screen of a computer flickers when the mobile phone is dialed in front of the computer. Especially, with the advent of the age of 5G, the living environment of people becomes more severe due to electromagnetic waves.
Electromagnetic shielding is one of effective means for suppressing electromagnetic interference and realizing electromagnetic protection. The upper-layer planning protection comprises reasonable industrial layout and strengthened regional control, so that an industrial area with intensive electronic and electrical equipment is far away from a residential area; and a green belt is arranged in a near-to-garden area to form a wave absorbing wall, so that the radiation of a field source to the surrounding environment is reduced. The absorption of the green plants to the electromagnetic radiation has the characteristics of wide frequency band, good effect and no negative influence. In terms of structural details, the electromagnetic wave shielding material can be used to isolate the shield from the shielded body, reducing the propagation of electromagnetic waves. A great deal of research is conducted in the scientific and industrial fields on electromagnetic wave shielding materials, generally metal good conductors or composite materials with low resistance, and when the electromagnetic wave reflectivity is required to be low or close to zero (wave absorption), the shielding materials are generally required to meet the conditions of impedance matching and the like. In the field of buildings, materials with electromagnetic wave shielding functions are applied, and the harm of electromagnetic waves to human bodies can be effectively reduced. Wherein the concrete wave-absorbing material as the main body structure is already applied in engineering. However, the cost is significantly increased by providing the shielding function to the main structure. If the waterproof material is endowed with a shielding function, the problem can be effectively solved. The waterproof material is used for the building envelope to prevent the penetration of rainwater, snow water and underground water; to prevent the erosion of moisture, steam and other harmful gases and liquids in the air; the partition structure is to prevent the permeation of the supply and drainage water. These materials that resist permeation, leakage and erosion are collectively referred to as water-resistant materials. The waterproof material is like a layer of coat and wraps the building to be protected.
The super-high grade polyester fiber cloth is modified to be conductive, and then the asphalt coiled material is prepared, so that the waterproof coiled material with the electromagnetic wave shielding function is obtained (CN 105584173A). Zhang hongbo et al modified the plastering mortar by using the conductive flexible fiber to prepare the electromagnetic shielding mortar (CN 104310907A). Polyurethane waterproof paint is one of important materials in waterproof materials, and is called liquid coiled material. Compared with coiled materials, the coiled materials have the advantages of convenience and rapidness in liquid construction, no need of open fire and the like, and can overcome the defects that the coiled materials cannot be used for construction of different parts and the like. Has great significance for the electromagnetic wave shielding functionalization of the polyurethane waterproof coating. At present, although there are many studies on electromagnetic wave shielding coatings, there has been no report on a polyurethane coating that can satisfy both the waterproof and electromagnetic wave shielding functions. Because the polyurethane waterproof coating needs to meet a certain elongation (specified in GB/T2965-2013 to be not less than 450%). As mentioned above, materials with electromagnetic wave shielding function usually have low resistance, and for this purpose, it is often necessary to add a large amount of conductive filler beyond the conductive threshold, however, the high content of conductive filler usually makes the mechanical properties of the composite material poor (brittle) and lacks extensibility; therefore, it is difficult to develop a polyurethane waterproofing paint having an electromagnetic wave shielding function and satisfying comprehensive properties such as extensibility of a conventional polyurethane waterproofing paint.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the polyurethane waterproof coating with the electromagnetic wave shielding function, so that the polyurethane waterproof coating has the electromagnetic wave shielding function and can meet the technical index requirements of the polyurethane waterproof coating.
In order to achieve the above object, a first aspect of the present invention provides a polyurethane waterproof coating material with an electromagnetic wave shielding function, which is prepared from the following raw materials in parts by weight: 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents;
wherein the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
The second method of the present invention provides a preparation method of the polyurethane waterproof coating, wherein the preparation method comprises:
(1) stirring and mixing the polyhydric alcohol, the plasticizer and the one-dimensional conductive filler, then adding the two-dimensional conductive filler and the optional pigment filler, continuously stirring and mixing, heating to 110-;
(2) cooling to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃ for continuous reaction, cooling to 45-75 ℃ again, optionally adding at least one of a chain extender, a solvent, a catalyst and other auxiliaries, and carrying out vacuum degassing to obtain the single-component polyurethane waterproof coating.
The third aspect of the present invention provides a preparation method of the above polyurethane waterproof coating, including:
preparation of component A: carrying out vacuum dehydration on the polyhydric alcohol at the temperature of 110-130 ℃, then reducing the temperature to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃, continuing to react, reducing the temperature to 45-75 ℃ again, and carrying out vacuum degassing to obtain a component A;
preparation of the component B: stirring and mixing the polyhydric alcohol, the plasticizer, the one-dimensional conductive filler and other optional additives and chain extenders, adding the two-dimensional conductive filler and optional pigments, continuously stirring and mixing, carrying out vacuum dehydration at the temperature of 110-130 ℃, then cooling to 45-75 ℃, optionally adding a catalyst and/or a solvent, and carrying out vacuum degassing to obtain the component B.
The technical scheme of the invention has the following beneficial effects:
(1) the invention functionalizes the waterproof material, solves the defect of single function of the waterproof material, and ensures that the prepared polyurethane waterproof coating has good electromagnetic shielding function.
(2) The waterproof coating provided by the invention has good electromagnetic shielding effect, and simultaneously has good comprehensive properties such as extensibility and strength.
(3) The invention can greatly reduce the harm of electromagnetic leakage caused by defects generated by electromagnetic shielding protection in the later period. And the invention can protect building owners from exposure to complex electromagnetic environments.
(4) The invention can meet the electromagnetic protection construction of the opposite part.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
Fig. 1 shows a schematic view of the conductive filler forming a conductive network in the waterproof coating material of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The first aspect of the invention provides a polyurethane waterproof coating with an electromagnetic wave shielding function, which is prepared from the following raw materials in parts by weight: 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents;
wherein the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
In the invention, preferably, the weight portions of the isocyanate monomer are 5 to 30 portions, the polyol is 20 to 95 portions, the conductive filler is 5 to 15 portions, the plasticizer is 10 to 40 portions, the pigment and filler is 10 to 50 portions, the chain extender is 0 to 5 portions, the solvent is 0 to 15 portions, and the catalyst is 0 to 0.5 portion.
According to the present invention, preferably, the polyurethane waterproof coating is a one-component polyurethane waterproof coating, and the one-component polyurethane waterproof coating includes: polyurethane prepolymer, conductive filler, plasticizer and optional pigment filler, chain extender, solvent, catalyst and other auxiliary agents; the polyurethane prepolymer is prepared by reacting an isocyanate monomer and polyol;
the composite material comprises, by weight, 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment and filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents;
the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
In the present invention, the weight portions of the isocyanate monomer are preferably 5 to 30 portions, more preferably 5 to 10 portions, the polyol is 20 to 95 portions, more preferably 20 to 50 portions, the conductive filler is 5 to 15 portions, the plasticizer is 10 to 40 portions, more preferably 10 to 20 portions, the pigment and filler is 10 to 50 portions, more preferably 10 to 35 portions, the chain extender is 0 to 5 portions, the solvent is 0 to 15 portions, and the catalyst is 0 to 0.5 portion, more preferably 0 to 0.1 portion.
According to the present invention, preferably, the polyurethane waterproof coating is a two-component polyurethane waterproof coating, and the two-component polyurethane waterproof coating comprises: a component A and a component B;
the component A is a polyurethane prepolymer which is prepared by reacting an isocyanate monomer and polyol;
the component B comprises: polyols, conductive fillers, plasticizers and optionally pigments, fillers, chain extenders, solvents, catalysts and other auxiliaries;
the composite material comprises, by weight, 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment and filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents; wherein the mass ratio of the polyhydric alcohol used in the component A to the polyhydric alcohol used in the component B is (2-27) to 1, preferably (8-19) to 1;
the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
In the present invention, the weight parts of the isocyanate monomer are preferably 5 to 30 parts, more preferably 10 to 30 parts, the polyol is 20 to 95 parts, more preferably 60 to 95 parts, the conductive filler is 5 to 15 parts, the plasticizer is 10 to 40 parts, more preferably 20 to 40 parts, the pigment and filler is 10 to 50 parts, more preferably 25 to 50 parts, the chain extender is 0 to 5 parts, the solvent is 0 to 15 parts, and the catalyst is 0 to 0.5 part, more preferably 0 to 0.3 part.
According to the present invention, preferably, the one-dimensional conductive filler includes carbon fibers and/or carbon nanotubes, preferably carbon nanotubes;
the two-dimensional conductive filler is conductive mica powder.
In the invention, the inventor researches and discovers that: the functional filler which is successfully applied as the electromagnetic wave shielding material at present is mainly metal filler due to higher electrical conductivity; however, the metal filler has the problems of high density, easy precipitation, easy oxidation of the surface, high price and the like; although there are reports on the application of carbon materials as electromagnetic wave shielding materials, most of the studies are limited to electromagnetic shielding function studies, and there are no studies on the influence of the addition of carbon materials on the elasticity, toughness, adhesion, etc. of waterproof coatings; the inventors of the present application found through studies that the carbon material cannot be added in the waterproof coating material too much, which would affect the properties of the waterproof coating material in terms of elasticity, toughness, adhesion, and the like, but the carbon material is not easily precipitated.
In conclusion, the invention aims to modify the polyurethane waterproof coating by using the functional conductive filler so as to meet the electromagnetic wave shielding and waterproof functions. Materials having an electromagnetic wave shielding function generally have low electrical resistance, and realization of the low electrical resistance often requires addition of a large amount of conductive filler. With the attendant embrittlement of the material. However, the waterproof material needs to have certain elastomeric characteristics. Therefore, a balance must be achieved between the two. The invention realizes the synergistic conduction effect by utilizing the two-dimensional conductive filler and the one-dimensional conductive filler. The two-dimensional conductive filler is conductive mica powder, and the one-dimensional conductive filler is carbon fiber and/or carbon nano tube. Because the existing waterproof paint formula system contains talcum powder, calcium carbonate, mica powder and the like, if the talcum powder, calcium carbonate, mica powder and the like are replaced by inorganic powder with a conductive function, the influence on the physical properties of the material is small. Meanwhile, a small amount of one-dimensional carbon nanotubes and/or carbon fibers are added, so that the formation of a conductive network can be promoted, the addition amount is small, and the influence on the viscosity of a system is small. Starting from the technical idea, the preparation of the waterproof coating with the electromagnetic wave shielding function is further realized. Fig. 1 shows a schematic diagram of a conductive network formed by conductive fillers in the waterproof coating material of the present invention, and as shown in fig. 1, one-dimensional conductive fillers play a role of bridging between two-dimensional conductive fillers, thereby greatly reducing the total addition amount of the fillers.
According to the present invention, preferably, the ratio of the length to the diameter of the one-dimensional conductive filler is > 100;
the average particle size of the two-dimensional conductive filler is 500-2000 meshes, and is preferably 1000-1500 meshes.
According to the present invention, preferably, the isocyanate monomer includes at least one of an aliphatic isocyanate, an aromatic isocyanate, an aliphatic isocyanate oligomer, and an aromatic isocyanate oligomer; the functionality of the aliphatic isocyanate and the aromatic isocyanate is not less than 2;
the aliphatic isocyanate is preferably at least one of isophorone diisocyanate (IPDI), dicyclohexylmethane diisocyanate (HMDI) and Hexamethylene Diisocyanate (HDI);
the aromatic isocyanate is preferably at least one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI) and tetramethylxylylene diisocyanate (TMXDI);
the aliphatic isocyanate oligomer and the aromatic isocyanate oligomer are respectively and independently dimer and/or trimer;
the isocyanate monomer is preferably Toluene Diisocyanate (TDI) and/or diphenylmethane diisocyanate (MDI);
the polyol comprises polyether polyol and/or polyester polyol; the functionality of the polyol is not less than 2; the weight average molecular weight of the polyol is 200-;
the polyol is preferably a polyether polyol having a weight average molecular weight of 2000 and/or a polyether polyol having a weight average molecular weight of 3000.
In the present invention, when preparing the two-component polyurethane waterproof coating material, the polyols used in the A, B component may be the same or different and are all selected from the above-defined polyols.
According to the present invention, preferably, the plasticizer includes at least one of chlorinated paraffin, dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, citrate-based plasticizer, vegetable oil ester-based plasticizer, sebacic acid ester-based plasticizer, and polyether polyol, preferably diisononyl phthalate (DINP) and/or chlorinated paraffin;
in the present invention, the polyether polyol as the plasticizer is at least one of a monofunctional polyether polyol and a polyether polyol having a functionality of two or more.
The catalyst is an organic metal catalyst, the organic metal catalyst is at least one of an organic tin catalyst, an organic zinc catalyst and an organic bismuth catalyst, and dibutyltin dilaurate (T-12) is preferred;
the pigment and filler comprises at least one of carbon black, titanium dioxide, iron oxide yellow, kaolin, cement, heavy calcium, barium sulfate, magnesium oxide, calcium oxide, wollastonite, silica micropowder, talcum powder and mica powder, and preferably calcium carbonate and/or talcum powder;
the chain extender comprises at least one of alcohols, amines and alcohol amines, preferably 3,3 '-dichloro-4, 4' -diphenylmethane diamine (MOCA) and/or diethylene glycol; the functionality of the chain extender is not less than 2;
the solvent comprises at least one of aromatic oil, toluene, xylene, 120# solvent oil, 150# solvent oil, ethyl acetate, butyl acetate, DMF and DMSO, and is preferably 150# solvent oil.
In the present invention, the solvent is an organic solvent, and is not particularly limited, and may be one or a mixture of more than one of any organic solvents in the field, and is preferably at least one of the organic solvents listed above; the solvent is selected from protic and/or aprotic solvents, preferably at least one of the organic solvents listed above.
According to the present invention, preferably, the other auxiliary agent includes at least one of a defoaming agent, a dispersing agent, a leveling agent, an anti-settling agent, a coupling agent, an antioxidant and a retarder;
the other auxiliary agents preferably comprise 0-0.5 part by weight of defoaming agent and 0-0.5 part by weight of dispersing agent.
In the present invention, the antifoaming agent is preferably BYK-065.
The second aspect of the present invention provides a preparation method of the above polyurethane waterproof coating, including:
(1) stirring and mixing the polyhydric alcohol, the plasticizer and the one-dimensional conductive filler, then adding the two-dimensional conductive filler and the optional pigment filler, continuously stirring and mixing, heating to 110-;
(2) cooling to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃ for continuous reaction, cooling to 45-75 ℃ again, optionally adding at least one of a chain extender, a solvent, a catalyst and other auxiliaries, and carrying out vacuum degassing to obtain the single-component polyurethane waterproof coating.
In the present invention, in the step (2), the reaction is preferably continued for 3 to 6 hours.
The third aspect of the present invention provides a preparation method of the above polyurethane waterproof coating, including:
preparation of component A: carrying out vacuum dehydration on the polyhydric alcohol at the temperature of 110-130 ℃, then reducing the temperature to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃, continuing to react, reducing the temperature to 45-75 ℃ again, and carrying out vacuum degassing to obtain a component A;
preparation of the component B: stirring and mixing the polyhydric alcohol, the plasticizer, the one-dimensional conductive filler and other optional additives and chain extenders, adding the two-dimensional conductive filler and optional pigments, continuously stirring and mixing, carrying out vacuum dehydration at the temperature of 110-130 ℃, then cooling to 45-75 ℃, optionally adding a catalyst and/or a solvent, and carrying out vacuum degassing to obtain the component B.
In the present invention, in the preparation of the component A, the reaction is preferably continued for 3 to 6 hours.
In the present invention, the water content of the vacuum-dehydrated material is preferably less than 500 ppm.
In the invention, when the two-component polyurethane waterproof coating is applied to construction, the mass ratio of the component A to the component B is preferably 1: 2-3.
The invention is further illustrated by the following examples:
the following examples and comparative examples all used raw materials in parts by weight.
The carbon nanotubes used in the following examples and comparative examples had a length of about 2 μm and a diameter of about 10 nm; the average grain diameter of the used conductive mica powder is 1250 meshes; the polyether polyols used have a functionality of 2 and/or 3;
polyether polyol C2020 available from wanhua chemical (nicotinerg) petrochemicals ltd, polyether polyol 330N available from tianjin petrochemicals ltd, polyether polyol DL1000 available from shanghai dongda chemical ltd; catalyst T-12 was purchased from air chemical; the defoaming agent is purchased from BYK company and has the brand number of BYK-065; dispersant BYK AT-203 was purchased from BYK.
Example 1
The embodiment provides a two-component polyurethane waterproof coating with an electromagnetic wave shielding function, and the preparation method comprises the following steps:
the preparation method of the component A comprises the following steps: putting 50 parts of polyether polyol (C2020) with the weight average molecular weight of 2000 and 35 parts of polyether polyol (330N) with the weight average molecular weight of 3000 into a three-necked bottle, starting stirring and starting vacuum, gradually heating to 120 ℃, timing after the temperature is reached, dehydrating in vacuum for 3 hours until the water content is below 500ppm, and starting cooling; cooling to 65 ℃, adding 15 parts of TDI, stirring for 30 minutes, heating to 85 ℃, and continuing to react for 3 hours; then cooling to 55 ℃, starting vacuum, degassing for 30 minutes, and discharging for later use.
The preparation method of the component B comprises the following steps: taking 30 parts of No. 52 chlorinated paraffin, 4.7 parts of 3000 weight-average molecular weight polyether polyol (330N), 4 parts of dispersant BYK AT-2030.5 parts, 2.8 parts of chain extender MOCA and 0.3 part of carbon nano tube in a three-neck flask, stirring and mixing for 30 minutes AT 2000r/min, then adding 8 parts of conductive mica powder and 49 parts of 800-mesh heavy calcium, continuing stirring and mixing, simultaneously starting vacuum, dehydrating for 3 hours AT 120 ℃, beginning to reduce the temperature to 60 ℃, adding 4.6 parts of catalyst T-120.1 and 150# solvent oil, stirring uniformly, degassing for 30 minutes in vacuum, and discharging for later use.
The component A and the component B are mixed according to the mass ratio of 1: 3 coating film with thickness of 1.5mm, curing for 7 days in standard environment (23 + -2 deg.C, humidity 50 + -10%), and testing.
Example 2
The embodiment provides a two-component polyurethane waterproof coating with an electromagnetic wave shielding function, and the preparation method comprises the following steps:
the preparation method of the component A comprises the following steps: putting 24 parts of polyether polyol (DL1000) with the weight average molecular weight of 1000, 43 parts of polyether polyol (C2020) with the weight average molecular weight of 2000 and 15 parts of polyether polyol (330N) with the weight average molecular weight of 3000 into a three-necked bottle, starting stirring and simultaneously starting vacuum, gradually raising the temperature to 120 ℃, timing after the temperature is reached, carrying out vacuum dehydration for 3 hours until the water content reaches below 500ppm, and starting cooling; cooling to 65 ℃, adding 18 parts of TDI, stirring for 30 minutes, heating to 85 ℃, and continuing to react for 3 hours; then cooling to 55 ℃, starting vacuum, degassing for 30 minutes, and discharging for later use.
The preparation method of the component B comprises the following steps: taking 32 parts of No. 52 chlorinated paraffin, 10 parts of polyether polyol (330N) with the weight average molecular weight of 3000, 3 parts of DINP plasticizer, 3 parts of dispersant BYK AT-2030.25 parts, 3.6 parts of chain extender MOCA and 0.7 part of carbon nano tube, stirring and mixing for 30 minutes AT 2000r/min, then adding 8 parts of conductive mica powder and 32 parts of 800-mesh heavy calcium, continuing stirring and mixing, simultaneously starting vacuum, dehydrating for 3 hours AT 120 ℃, starting to cool to 60 ℃, adding catalyst T-120.2 parts and 10.25 parts of 150# solvent oil, stirring uniformly, degassing for 30 minutes in vacuum, and discharging for later use.
The component A and the component B are mixed according to the mass ratio of 1: 2.5 coating film with the thickness of 1.5mm, curing for 7 days in a standard environment (23 +/-2 ℃ and humidity of 50 +/-10 percent), and testing.
Example 3
The embodiment provides a single-component polyurethane waterproof coating with an electromagnetic wave shielding function, and the preparation method comprises the following steps: taking 30.2 parts of polyether polyol (C2020) with the weight-average molecular weight of 2000, 4 parts of polyether polyol 330N (with the weight-average molecular weight of 4800), 8 parts of chlorinated paraffin, 10.41 parts of DINP, adding 0.5 part of carbon nano tube, stirring and mixing for 30 minutes at 2000r/min, then adding 12 parts of conductive mica powder and 30 parts of 800-mesh heavy calcium, continuing stirring and mixing for 30 minutes, heating to 120 ℃, performing vacuum dehydration for 3 hours, cooling to 60 ℃ after the water content is lower than 300ppm, adding 5.7 parts of TDI, stirring and mixing for 30 minutes, heating to 85 ℃, and continuing to react for 3 hours; cooling to 60 ℃, adding 0.5 part of defoaming agent and 0.06 part of T-12, stirring uniformly, and then vacuum degassing for 30 minutes to obtain the product for later use.
Coating film with thickness of 1.5mm, maintaining for 7 days in standard environment (23 + -2 deg.C, humidity 50 + -10%), and testing.
Example 4
The embodiment provides a single-component polyurethane waterproof coating with an electromagnetic wave shielding function, and the preparation method comprises the following steps: taking 30 parts of polyether polyol (with the weight-average molecular weight of 2000, C2020), 4 parts of polyether polyol 330N (with the weight-average molecular weight of 4800) and 18 parts of DINP, adding 1 part of carbon nano tube, stirring and mixing for 30 minutes at 2000r/min, then adding 10 parts of conductive mica powder and 25 parts of 800-mesh heavy calcium, continuing stirring and mixing for 30 minutes, heating to 120 ℃, performing vacuum dehydration for 3 hours, cooling to 60 ℃, adding 5.8 parts of TDI, stirring and mixing for 30 minutes, heating to 85 ℃, continuing to react for 3 hours, cooling to 60 ℃, adding 0.5 part of defoaming agent, 0.06 part of T-12 and 7.5 parts of No. 150 solvent oil, uniformly stirring, performing vacuum degassing for 30 minutes, and taking out for later use.
Coating film with thickness of 1.5mm, maintaining for 7 days in standard environment (23 + -2 deg.C, humidity 50 + -10%), and testing.
Comparative example 1
The comparative example is different from the example 1 only in that 8 parts of the conductive mica powder is replaced by 8 parts of graphene, and the rest is the same as the example 1.
The component A and the component B are mixed according to the mass ratio of 1: 3 coating film with thickness of 1.5mm, curing for 7 days in standard environment (23 + -2 deg.C, humidity 50 + -10%), and testing.
Comparative example 2
The comparative example is different from example 3 only in that 12 parts of conductive mica powder is replaced by 12 parts of graphene, and the rest is the same as example 1.
Test example
The polyurethane waterproof coatings prepared in the above examples and comparative examples were subjected to performance tests, and specific test results are shown in table 1.
TABLE 1 results of sample testing
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (14)
1. A polyurethane waterproof coating with an electromagnetic wave shielding function is characterized in that the raw materials for preparing the polyurethane waterproof coating comprise, by weight: 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents;
wherein the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30);
the one-dimensional conductive filler comprises carbon fibers and/or carbon nanotubes;
the two-dimensional conductive filler is conductive mica powder.
2. The polyurethane waterproof coating material according to claim 1, wherein the polyurethane waterproof coating material is a one-component polyurethane waterproof coating material comprising: polyurethane prepolymer, conductive filler, plasticizer and optional pigment filler, chain extender, solvent, catalyst and other auxiliary agents; the polyurethane prepolymer is prepared by reacting an isocyanate monomer and polyol;
the composite material comprises, by weight, 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment and filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents;
the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
3. The polyurethane waterproofing coating according to claim 1, wherein the polyurethane waterproofing coating is a two-component polyurethane waterproofing coating, and the two-component polyurethane waterproofing coating comprises: a component A and a component B;
the component A is a polyurethane prepolymer which is prepared by reacting an isocyanate monomer and polyol;
the component B comprises: polyols, conductive fillers, plasticizers and optionally pigments, fillers, chain extenders, solvents, catalysts and other auxiliaries;
the composite material comprises, by weight, 5-95 parts of isocyanate monomer, 5-95 parts of polyol, 0.5-70 parts of conductive filler, 1-50 parts of plasticizer, 0-50 parts of pigment and filler, 0-10 parts of chain extender, 0-20 parts of solvent, 0-1 part of catalyst and 0-1 part of other auxiliary agents; wherein the mass ratio of the polyol used in the component A to the polyol used in the component B is (2-27) to 1;
the conductive filler comprises a one-dimensional conductive filler and a two-dimensional conductive filler; the mass ratio of the one-dimensional conductive filler to the two-dimensional conductive filler is 1 (8-30).
4. The polyurethane waterproofing coating according to any one of claims 1 to 3, wherein the one-dimensional conductive filler is a carbon nanotube.
5. The polyurethane waterproofing coating according to any one of claims 1 to 3, wherein the ratio of the length to the diameter of the one-dimensional conductive filler is > 100;
the average particle size of the two-dimensional conductive filler is 500-2000 meshes.
6. The polyurethane waterproof coating material as claimed in claim 5, wherein the average particle size of the two-dimensional conductive filler is 1000-1500 mesh.
7. The polyurethane waterproofing coating according to any one of claims 1 to 3, wherein the isocyanate monomer includes at least one of an aliphatic isocyanate, an aromatic isocyanate, an aliphatic isocyanate oligomer, and an aromatic isocyanate oligomer; the functionality of the aliphatic isocyanate and the aromatic isocyanate is not less than 2;
the aliphatic isocyanate oligomer and the aromatic isocyanate oligomer are each independently a dimer and/or trimer.
8. The polyurethane waterproofing coating according to claim 7,
the aliphatic isocyanate is at least one of isophorone diisocyanate, dicyclohexyl methane diisocyanate and hexamethylene diisocyanate;
the aromatic isocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate and tetramethylxylylene diisocyanate;
the isocyanate monomer is toluene diisocyanate and/or diphenylmethane diisocyanate;
the polyol is polyether polyol with the weight-average molecular weight of 2000 and/or polyether polyol with the weight-average molecular weight of 3000.
9. The polyurethane waterproof coating material according to any one of claims 1 to 3, wherein the plasticizer includes at least one of chlorinated paraffin, dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, a citrate-based plasticizer, a vegetable oil-based plasticizer, a sebacic ester-based plasticizer, and a polyether polyol;
the catalyst is an organic metal catalyst, and the organic metal catalyst is at least one of an organic tin catalyst, an organic zinc catalyst and an organic bismuth catalyst;
the pigment and filler comprises at least one of carbon black, titanium dioxide, iron oxide yellow, kaolin, cement, heavy calcium, barium sulfate, magnesium oxide, calcium oxide, wollastonite, silica micropowder, talcum powder and mica powder;
the chain extender comprises at least one of alcohols, amines and alcohol amines; the functionality of the chain extender is not less than 2;
the solvent comprises at least one of aromatic oil, toluene, xylene, No. 120 solvent oil, No. 150 solvent oil, ethyl acetate, butyl acetate, DMF and DMSO.
10. The polyurethane waterproof coating material according to claim 9,
the plasticizer is diisononyl phthalate and/or chlorinated paraffin;
the organic metal catalyst is dibutyltin dilaurate;
the pigment and filler is calcium carbonate and/or talcum powder;
the chain extender is 3,3 '-dichloro-4, 4' -diphenylmethane diamine and/or diethylene glycol;
the solvent is 150# solvent oil.
11. The polyurethane waterproofing coating according to any one of claims 1 to 3, wherein the other auxiliary agent comprises at least one of an antifoaming agent, a dispersing agent, a leveling agent, an anti-settling agent, a coupling agent, an antioxidant, and a retarder.
12. The polyurethane waterproof coating material according to claim 11, wherein the other auxiliary agent comprises 0 to 0.5 parts by weight of a defoaming agent and 0 to 0.5 parts by weight of a dispersing agent.
13. A method for preparing the polyurethane waterproofing paint according to any one of claims 1 to 12, characterized in that the method comprises:
(1) stirring and mixing the polyhydric alcohol, the plasticizer and the one-dimensional conductive filler, then adding the two-dimensional conductive filler and the optional pigment filler, continuously stirring and mixing, heating to 110-;
(2) cooling to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃ for continuous reaction, cooling to 45-75 ℃ again, optionally adding at least one of a chain extender, a solvent, a catalyst and other auxiliaries, and carrying out vacuum degassing to obtain the single-component polyurethane waterproof coating.
14. A method for preparing the polyurethane waterproofing paint according to any one of claims 1 to 12, characterized in that the method comprises:
preparation of component A: carrying out vacuum dehydration on the polyhydric alcohol at the temperature of 110-130 ℃, then reducing the temperature to 45-75 ℃, adding an isocyanate monomer, stirring and mixing, heating to 80-90 ℃, continuing to react, reducing the temperature to 45-75 ℃ again, and carrying out vacuum degassing to obtain a component A;
preparation of the component B: stirring and mixing the polyhydric alcohol, the plasticizer, the one-dimensional conductive filler and other optional additives and chain extenders, adding the two-dimensional conductive filler and optional pigments, continuously stirring and mixing, carrying out vacuum dehydration at the temperature of 110-130 ℃, then cooling to 45-75 ℃, optionally adding a catalyst and/or a solvent, and carrying out vacuum degassing to obtain the component B.
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| CN113462293A (en) * | 2021-07-02 | 2021-10-01 | 河北三棵树涂料有限公司 | Silane modified resin waterproof coating and preparation method thereof |
| CN116496690A (en) * | 2022-10-12 | 2023-07-28 | 中国航发北京航空材料研究院 | High-elasticity high-toughness low-frequency radar wave-absorbing material and preparation method thereof |
| CN117186623B (en) * | 2023-09-11 | 2024-02-13 | 昆山红苹果塑胶新材料有限公司 | Heat-resistant stable TPU film and preparation method thereof |
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